A study of the behaviour of some new column materials in the chromatographic analysis of Cinchona alkaloids

Summary A major problem in the HPLC analysis of alkaloids is the poor peak shape and consequently low resolution, due to the interactions of the basic alkaloids with the residual acidic silanol groups of most reversed phase materials. The performance of new packing materials specially designed for the separation of basic compounds has been studied using mobile phases without the special additives commonly applied in the analysis of alkaloids. Strongly basic Cinchona alkaloids were used as test compounds. Retention characteristics and selectivities of each material were studied, after mobile phase optimisation for the column. The influence of the major factors (nature and content of the organic modifier, pH value, salt concentration) affecting resolution was studied. The mobile phases were chosen so that they could be used in thermospray LC-MS. The addition of salts to the mobile phase improves separation but in general the modification of the mobile phase gave little change in selectivity. The performance of silicabased C₁₈ material proved superior to the polymer materials tested.     

毛细管气相色谱法快速测定羰基合成脂肪醇中的正构醇

The normal alcohols in fatty alcohols produced from hydroformylation unit were determined directly byOV-1 capillary GC method; This method is simple,rapid and accurate。The relative error is below 2%andcoefficient of variation is below 3%。     

高温毛细管气相色谱柱的制备及应用

研究了臭氧交联法制备毛细管气相色谱柱的方法,即用镀铝石英毛细管,涂渍ＳＥ３１,经臭氧交联,最高使用温度可达３６０℃。测试的结果表明其柱效高,吸附性小,热稳定性好,适用于烃类、醇类、多环芳烃及二硝基甲苯和三硝基甲苯的分离。     

气相色谱专家系统的进展

综述了国家色谱研究分析中心在气相色谱专家系统方面的进展,着重于色谱分离模式的推荐、气相色谱柱系统的推荐、气相色谱操作条件的最佳化、气相色谱在线定性定量分析四个方面;列举了在石化部门和环境监测中气相色谱专家系统应用的大量成功实例,以说明软件的实用性。     

富勒烯C60的柱色谱分离法研究

本文提出了由Ｃ（６０）、Ｃ（７０）及少量高级富勒烯混合物（来自电弧汽化石墨所形成的碳灰）中分离出纯度为９９．９％Ｃ（６０）的两种改进的、简便价廉的柱色谱分离法．第一种方法用中性氧化铝作固定机以石油醚与甲苯（Ｖ／Ｖ＝９２．５／７．５）混合液作流动相；另一种方法以活性炭与硅胶作固定相，以甲苯作流动相，柱顶氮压约为０．０１ａｔｍ．本文尚将这两种方法与文献报道的两种相近的方法分别进行了比较．     

烯唑醇免疫亲和色谱柱的制备及其在样品前处理中的应用

将四甲氧基硅烷(TMOS)水解后与烯唑醇抗体聚合,采用溶胶-凝胶法合成了烯唑醇免疫亲和色谱(IAC)柱固定相,并用其制备了对烯唑醇具有特异性亲和力的IAC柱。对IAC柱条件进行了优化,选择超纯水作为吸附与平衡介质,30%～50%(体积分数)甲醇水溶液作为洗脱剂。结果表明: 在优化条件下,IAC柱对烯唑醇的动态柱容量达125.4 μg/g。在河水样品和水果样品中添加烯唑醇,经IAC柱净化富集,洗脱液采用高效液相色谱检测,河水中烯唑醇的平均回收率为90.36%～100.14%,相对标准偏差(RSD)为2.03%～6.08%;水果中烯唑醇的平均回收率为85.55%～94.02%, RSD为3.38%～6.78%。本研究为烯唑醇在河水、水果等样品中的残留分析提供了一种新的高效前处理手段。     

A modified simplex method for multifactor optimization of selectivity in gas chromatography

A computer-assisted advanced simplex method is presented for the simultaneous optimization of multifactor ( stationary phase loading, carrier gas flow rate and column temperature ) for separation of ten compounds in gas chromatography. A three factors factorial design was used. The method was based on a special polynomial established from fifteen preliminary runs, using resolution as the selection criterion, with connection to a general simplex method. Excellent agreement is found between the predicted data and the experimental results, and most of experiments required in the general simplex method can be omitted.     

双苯甲酰胺冠醚固定相的合成及毛细管柱气相色谱性能的研究

合成了一种新型的双苯甲酰胺冠醚固定相:(1S,2S)-1-(对苯甲酰胺基)苯基-2-苯甲酰胺基-16-冠-5,其结构经红外光谱、核磁共振、质谱及元素分析数据证实。考察了这种固定相的柱效、热稳定性、极性及选择性等色谱特性。该类固定相对极性位置异构体分离效果良好。由于冠醚上引入苯甲酰胺取代基,因而对苯胺类及不经衍生化的碱性化合物能特殊选择性地分离。     

顶空气相色谱法测定延生护宝液中甲醇残留量

本文用顶空气相色谱法，以ＧＤＸ－１０１为固定相，测定了延生护宝液中甲醇残留量，方法的回收率在８５．９％－１０１．６％之间，变异系数０．３％，最小检出量１．０ｍｇ／Ｌ。     

苯酚、马尿酸和甲基马尿酸的反相高效液相色谱分析

本文提出了人体内苯、甲苯和二甲苯的代谢产物苯酚、马尿酸和甲基马尿酸的反相高效液相色谱分析法,讨论了其保留机制和样品预处理技术.以ODS为固定相,甲醇-水-醋酸为流动相时可实现良好分离.方法回收率为97.3%,相对标准偏差为1.02%.提出的方法可用于尿样分析,适用于临床与职业病防治的监测分析.